Corrosion Behavior and Mechanism of Low Activation 9Cr-ODS Steel in High Temperature and High Pressure Water Environment for the Application in Fusion Reactors

doi:10.11900/0412.1961.2023.00465

Acta Metall Sin

2025, Vol. 61

Issue (9): 1305-1319 DOI: 10.11900/0412.1961.2023.00465

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Corrosion Behavior and Mechanism of Low Activation 9Cr-ODS Steel in High Temperature and High Pressure Water Environment for the Application in Fusion Reactors

FU Haiyang¹^,², ZHANG Jiarong¹^,³(

), LI Yaozhi¹^,², WANG Qitao¹^,², LI Xinle¹^,², YAN Wei¹^,³, SHAN Yiyin¹^,³, LI Yanfen¹^,³(

)

1 Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2 School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China
3 CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

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FU Haiyang, ZHANG Jiarong, LI Yaozhi, WANG Qitao, LI Xinle, YAN Wei, SHAN Yiyin, LI Yanfen. Corrosion Behavior and Mechanism of Low Activation 9Cr-ODS Steel in High Temperature and High Pressure Water Environment for the Application in Fusion Reactors. Acta Metall Sin, 2025, 61(9): 1305-1319.

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Abstract

The China fusion engineering test reactor is a bridge between the international thermonuclear experimental reactor and future fusion demonstration reactors. The harsh service environment of the fusion reactor, including high heat flow density, strong neutron irradiation, and high temperature and high pressure coolant corrosion, demands higher requirements on structural materials than conventional nuclear energy structural materials. Low activation oxide dispersion-strengthened (ODS) steels, which are developed based on reduced activation ferritic/martensitic steels, are considered as promising candidate fusion reactor structural materials because of their high creep strength and excellent resistance to irradiation. In this study, 9Cr-ODS steel prepared by mechanical alloying (MA) and Chinese low activated martensitic (CLAM) steel prepared by vacuum smelting were selected because of their excellent mechanical properties and superior radiation tolerance. The main difference between the two steels is the grain size: the average grain size of the 9Cr-ODS steel is 200-500 nm, whereas that of CLAM steel is 10-20 μm. Furthermore, the 9Cr-ODS steel was added with Y₂O₃ during MA, which improved its mechanical properties and thermal stability. Corrosion experiments were conducted in static and dynamic (flow rate of 5 mL/min) ultrapure water at 325 ^oC and 15.5 MPa. Ultrapure water had an electrical conductivity of 0.1 μS/cm and a dissolved oxygen content of 10 × 10^-9. The exposure time for both steels were set as 200, 500, and 1000 h. Results indicated that under static and dynamic conditions, the corrosion mass gain and oxide film thickness of the 9Cr-ODS steel were less than those of the CLAM steel. Under static conditions, the corrosion product of both materials exhibits a double-layer structure with granular Fe₃O₄ in the outer layer and continuous Cr- and Fe-rich spinel in the inner layer. As the exposure time increased from 200 h to 1000 h, the size and thickness of the oxide particles gradually increased. However, under dynamic conditions with a flow rate of 5 mL/min, the surface of the 9Cr-ODS steel formed not only Fe₃O₄ but also a small amount of Fe₂O₃, while the type of oxide in the outer layer of the CLAM steel remains unchanged. In contrast to the static condition, both steels exhibited decreased corrosion mass loss and oxide film thickness because of the dynamic water scouring effect and the buildup of H₂ on the surface caused by water decomposition through oxidation. Overall, under same corrosion conditions, the presence of dispersed oxides, grain refinement, and a high matrix oxygen concentration positively enhanced the corrosion resistance of the 9Cr-ODS steel. This enhancement facilitated the formation of a protective inner oxide layer and reduced the corrosion mass loss rate, thereby demonstrating the superior corrosion resistance of the 9Cr-ODS steel under high temperature and high pressure water environments compared with the CLAM steel.

Key words: low activation ODS steel high temperature and high pressure water corrosion oxide film

Received: 29 November 2023

ZTFLH:

TG172.82

Fund: National Natural Science Foundation of China(51971217);National Magnetic Confinement Fusion Science Program of China(2019YFE03130000);Strategic Priority Research Program of the Chinese Academy of Sciences(XDA0410000)

Corresponding Authors: LI Yanfen, professor, Tel: (024)23978990, E-mail: yfli@imr.ac.cn;
ZHANG Jiarong, Tel: (024)83973136, E-mail: jrzhang14s@imr.ac.cn

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	FU Haiyang
	ZHANG Jiarong
	LI Yaozhi
	WANG Qitao
	LI Xinle
	YAN Wei
	SHAN Yiyin
	LI Yanfen

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https://www.ams.org.cn/EN/10.11900/0412.1961.2023.00465 OR https://www.ams.org.cn/EN/Y2025/V61/I9/1305

Table 1 Chemical compositions of 9Cr-ODS and (CLAM) steels

Table 2 Heat treatment processes for 9Cr-ODS and CLAM steels

Fig.1 Schematic of corrosion test circuitt device

Fig.2 EBSD maps showing matrix grain size of 9Cr-ODS steel (a) and CLAM steel (b)

Fig.3 Oxidation mass gain (ΔW) curves of 9Cr-ODS and CLAM steels in static and dynamic high temperature and high pressure water (t—time)

Fig.4 XRD spectra of 9Cr-ODS and CLAM steels after corrosion in static (a) and dynamic (b) high temperature and high pressure water

Fig.5 Surface corrosion product SEM images of 9Cr-ODS (a-c) and CLAM (d-f) steels after corrosion in static condition for 200 h (a, d), 500 h (b, e), and 1000 h (c, f)

Table 3 EDS results of the marked points in Fig.5

Fig.6 Surface corrosion product SEM images of 9Cr-ODS (a-c) and CLAM (d-f) steels after corrosion in dynamic condition for 200 h (a, d), 500 h (b, e), and 1000 h (c, f)

Table 4 EDS results of the marked points in Fig.6

Fig.7 Detailed XPS of Fe on the outer surface of 9Cr-ODS (a, c) and CLAM (b, d) steels after corrosion in static (a, b) and dynamic (c, d) high temperature and high pressure water for 1000 h

Fig.8 Fe2p_3/2 NLS fitting results of 9Cr-ODS steel after corrosion in static high temperature and high pressure water for 1000 h (NLS—non-linear least squares)

Fig.9 Detailed XPS of Cr on the outer surface of 9Cr-ODS (a, c) and CLAM (b, d) steels after corrosion in static (a, b) and dynamic (c, d) high temperature and high pressure water for 1000 h

Fig.10 Cross-sectional SEM images of corrosion products of 9Cr-ODS (a-c) and CLAM (d-f) steels after corrosion in static high temperature and high pressure water for 200 h (a, d), 500 h (b, e), and 1000 h (c, f)

Fig.11 Cross-sectional SEM images showing corrosion product morphologies of 9Cr-ODS (a-c) and CLAM (d-f) steels after corrosion in dynamic high temperature and high pressure water for 200 h (a, d), 500 h (b, e), and 1000 h (c, f)

Fig.12 Cross-sectional SEM images and EPMA element maps of 9Cr-ODS steel after corrosion in static (a) and dynamic (b) high temperature and high pressure water for 1000 h

Fig.13 Cross-sectional TEM image (a) of oxide film of 9Cr-ODS steel after corrosion in dynamic high temperature and high pressure water for 1000 h, and corresponding SAED patterns of zone A (b) and zone B (c) in Fig.13a

No.	Formation	$Δ G 0 = R T l n p O 2$ / (kJ·mol^-1·O₂^-1)
1	$4 F e 3 O 4 + O 2 = 6 F e 2 O 3$	-327.801
2	$43 F e + O 2 = 23 F e 2 O 3$	-446.466
3	$32 F e + O 2 = 12 F e 3 O 4$	-461.299
4	$2 F e + 2 C r 2 O 3 + O 2 = 2 F e C r 2 O 4$	-600.519
5	$12 F e + C r + O 2 = 12 F e C r 2 O 4$	-654.714
6	$43 C r + O 2 = 23 C r 2 O 3$	-672.778

Table 5 Calculation results of standard Gibbs free energies of oxide formation on the steel surface at 325 ^oC and 25 MPa

Fig.14 Schematics of corrosion process of 9Cr-ODS steel in static and dynamic high temperature and high pressure water
(a) early stage of corrosion (b) static (c) dynamic

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